CN102557970B - Preparation method of anhydrous betaine - Google Patents
Preparation method of anhydrous betaine Download PDFInfo
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- CN102557970B CN102557970B CN201010606019.2A CN201010606019A CN102557970B CN 102557970 B CN102557970 B CN 102557970B CN 201010606019 A CN201010606019 A CN 201010606019A CN 102557970 B CN102557970 B CN 102557970B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 4
- 229940023579 anhydrous betaine Drugs 0.000 title abstract 3
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims abstract description 49
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 29
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 16
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000009835 boiling Methods 0.000 claims abstract description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000000909 electrodialysis Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 25
- 238000002425 crystallisation Methods 0.000 claims description 21
- 230000008025 crystallization Effects 0.000 claims description 21
- 238000004519 manufacturing process Methods 0.000 claims description 20
- 229950010582 betaine anhydrous Drugs 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 16
- 235000016068 Berberis vulgaris Nutrition 0.000 claims description 14
- 241000335053 Beta vulgaris Species 0.000 claims description 14
- 239000003513 alkali Substances 0.000 claims description 14
- NJZRLXNBGZBREL-UHFFFAOYSA-N glycine betaine hydrate Chemical compound [OH-].C[N+](C)(C)CC(O)=O NJZRLXNBGZBREL-UHFFFAOYSA-N 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000013078 crystal Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000011344 liquid material Substances 0.000 claims description 12
- 238000010612 desalination reaction Methods 0.000 claims description 11
- 239000012141 concentrate Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000011552 falling film Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 235000011089 carbon dioxide Nutrition 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 230000001351 cycling effect Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000001704 evaporation Methods 0.000 abstract description 3
- 229960003237 betaine Drugs 0.000 abstract description 2
- 230000018044 dehydration Effects 0.000 abstract description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 2
- 238000011033 desalting Methods 0.000 abstract 4
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 abstract 1
- 229940106681 chloroacetic acid Drugs 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 235000008504 concentrate Nutrition 0.000 description 7
- 241000196324 Embryophyta Species 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 101100476962 Drosophila melanogaster Sirup gene Proteins 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- 150000007854 aminals Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 235000009508 confectionery Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
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- 239000000284 extract Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 150000003385 sodium Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method for preparing anhydrous betaine through chemical synthesis. High-purity anhydrous betaine of which the purity is over 99.9 percent is produced by performing procedures including neutralizing, substituting, concentrating, primary desalting, secondary desalting, evaporating, crystalizing, centrifuging, drying and the like on chloroacetic acid, sodium carbonate and trimethylamine serving as major raw materials through a process for combining electrodialysis desalting, evaporative desalting and a boiling dryer. In the process, the original methanol dehydration and double-core dryer drying equipment is eliminated, and obtained metahydrate betaine is directly dried by using a boiling drier, so that cost on each ton can be saved by about 1,200 yuan, and the yield is increased by 3 tons per day.
Description
Technical field
The present invention relates to a kind of production technique being prepared BETAINE anhydrous by chemosynthesis, particularly relate to a kind of Mono Chloro Acetic Acid, sodium carbonate, Trimethylamine 99 be the production technique that main raw material prepares BETAINE anhydrous.
Background technology
Trimethyl-glycine is a kind of natural biostearin material, molecular formula (CH
3)
3nCH
2cOO, molecular weight 117, nontoxic, water absorbability is extremely strong, taste is sweet, have special odor, and it is extensively formed in the bodies of aminal and plant and has important function, its be worth by countless scientific researches, practice affirm.The purposes of trimethyl-glycine widely.Such as, in medical, trimethyl-glycine can be used for medicine, the antibiotic raw material of production for treating and prevention hepatopathy.Trimethyl-glycine can be used as foodstuff additive, can play good promoter action to care of aged, upgrowth and development of children.In daily-use chemical industry, because trimethyl-glycine character is extremely gentle, be excellent permeate agent, wetting Agent for Printing Inks and sweeting agent, thus can add in shampoo, body lotion, hair conditioner, skin care green grass or young crops and toothpaste.To the severe plant as dry morning, high salt, high temperature, high humidity etc. of growth conditions or the exogenous betaine administration of crop can promote they growth, improve their output.
The method preparing trimethyl-glycine at present mainly contains two kinds: one extracts from beet sirup fermented liquid, its extraction process mainly ion exclusion method, using polythene-styrene chromatography column, the trimethyl-glycine mother liquor eluted, through evaporation, concentrated, three sections of crystallizations, filters the anhydrous or trimethylglycine hydroxide of obtained purity about 98%.Present method is subject to the restriction in season and area, and extraction process is also more loaded down with trivial details.Another kind is prepared by chemical synthesis process, adopt Mono Chloro Acetic Acid and Trimethylamine 99 to be that raw material carries out reaction generation trimethyl-glycine and sodium-chlor in alkali lye, but the sodium-chlor that reaction generates is difficult to removing.Chinese patent CN93109224 discloses a kind of strong-acid ion exchange resin that adopts and adsorbs, weak ammonia desorb, then concentrate, the purification desalination method of crystallization, the shortcoming of this method is not only complex process, and the production cycle is long, and efficiency is low, and energy consumption is very large, during ion exchange resin regeneration, also has a large amount of discharge of wastewater.
Trimethyl-glycine and hydrochloride thereof are when being prepared by chemical synthesis process, and owing to limitting by some specific synthesis condition, will inevitably produce a large amount of by product monochlor(in)ate sodium, sodium-chlor and principal product generate simultaneously, are doped in principal product.Meanwhile, also have a small amount of heavy metal substance to be mixed in product.These impurity destroy the quality of principal product trimethyl-glycine all greatly, it must be separated removing completely.How to accomplish to be separated the most thoroughly, be the important subject of trimethyl-glycine industry always.
Through finding with statistics the deep market study of domestic and international manufacturing enterprise, present trimethyl-glycine, what beet alkali hydrochlorate manufacturing enterprise generally adopted prepares extracting method, ubiquity adulterates wherein as by product in product thus causes the problems such as foreign matter content is high, constrain enterprise development to a certain extent, the anhydrous type crystallization trimethyl-glycine of the vacuum distilling method DNA purity 98% generally used as domestic, the most outstanding defect of the method is, during owing to distilling, the viscosity of mother liquor is more and more higher, and sodium-chlor solubility with temperature change is in the solution also little, side product chlorinated sodium is caused effectively all not to be separated with principal product, the method is to the requirement of technical controlling height very, generally can not obtain highly purified BETAINE anhydrous.Ion exchange method comparatively advanced at present can improve the deficiency of vacuum distillation method to a certain extent, but the method cost is high, and is not suitable for large-scale industrialization production running.And the invention provides a kind of brand-new Production Flow Chart, with ordinary method ratio have invest low, product purity is high, raw material consumption amount is low, cost-saving, improve the advantages such as production capacity, thus has good promotional value.
Summary of the invention
The invention provides a kind of BETAINE anhydrous production technique, be intended to solve the problems such as the ubiquitous investment of existing BETAINE anhydrous production technique is large, product purity is low, production capacity is low, present method is significant to propelling large-scale production.
Technical scheme of the present invention is:
1, a BETAINE anhydrous production technique, is characterised in that and comprises the following steps:
(1) under normal temperature by 2 tons of water, 1.5 tons of Mono Chloro Acetic Acids, 0.84 ton of sodium carbonate drops in reactor, will note rate of feeding, be as the criterion not separate out a large amount of carbonic acid gas when feeding intake;
(2) finish after material fully reacts and pass into 0.95 ton of Trimethylamine 99 again, when feeding intake, temperature of reaction controls at 55-65 DEG C, stop as PH=7 feeding intake, Trimethylamine 99 feeds intake in process, reactor pressure does not allow more than 0.1Mpa, and after the logical material of Trimethylamine 99, temperature 50-60 DEG C starts to stir, be incubated 3 hours, then material moves in concentration response still;
(3) make vapor pressure be stabilized in 0.3MPa, concentrate to heating material, vacuum pressure is stabilized in-0.08MPa, heating is stopped when temperature of charge reaches 115 DEG C, stir 20 minutes, then supernatant liquor moves in liquid material hold-up vessel, and the every five batches of cleanings of the sodium-chlor in reactor once;
(4) supernatant liquor adds pure water to be diluted to salts contg is less than 10 % by weight, desalination is carried out through electrodialysis appts after mixing of materials is even, the alkali solution of beet ash of output is not more than 0.5 % by weight, detect qualified after, the salts solution of output is beaten in salts solution hold-up vessel;
(5) alkali solution of beet falling film condenser concentrates, make vapor pressure be stabilized in 0.3MPa, vacuum pressure is stabilized in-0.08MPa, stops heating when temperature of charge reaches 115 DEG C, concentrated end, the alkali solution of beet after then concentrating moves in trimethyl-glycine crystallization kettle;
(6) trimethyl-glycine crystallization: the trimethyl-glycine liquid material cooling in concentrated post crystallization still, make temperature of charge be down to less than 10 DEG C, xln is separated out in a large number;
(7) trimethyl-glycine is centrifugal: carry out solid-liquid separation with whizzer, the crystallization of output trimethylglycine hydroxide, ash is not more than 0.1 % by weight, detect qualified after, the trimethylglycine hydroxide crystal produced loads in the material cycling bag of regulation, isolated liquid collecting is in liquid material holding tank, and production cycle is applied mechanically;
(8) dropped in boiling drier by trimethylglycine hydroxide crystal, temperature controls below 115 DEG C, dry 20-30 minute, the crystal water in product and moisture is dried, obtains BETAINE anhydrous product.
The falling film condenser used is the manufacture of Shandong Zibo Sheng Xin graphite equipment company limited.
The invention has the beneficial effects as follows: utilize Mono Chloro Acetic Acid, sodium carbonate, Trimethylamine 99 is main raw material, through neutralization, replace, concentrated, a desalination, secondary desalination, evaporation, crystallization, centrifugal, the operations such as drying, the explained hereafter combined by electrodialysis desalination and evaporative desalination and boiling drier goes out more than 99.9% highly purified BETAINE anhydrous, this technique eliminates original existing methanol dehydration and two vertebra drying machine drying plant, after obtaining trimethylglycine hydroxide, direct boiling drier is dried, cost-saved about 1200 yuan per ton, improve production capacity 3 tons/day.
Accompanying drawing explanation
Fig. 1 is the schema of BETAINE anhydrous production technique of the present invention, wherein relate generally to and use Mono Chloro Acetic Acid, sodium carbonate, Trimethylamine 99 to be raw material, through reaction, concentrated, desalination, secondary desalination, secondary concentration, crystallization, separation, finally obtain BETAINE anhydrous.
Embodiment
Embodiment 1
(1) under normal temperature by 2 tons of water, 1.5 tons of Mono Chloro Acetic Acids, 0.84 ton of sodium carbonate drops in reactor, will note rate of feeding, be as the criterion not separate out a large amount of carbonic acid gas when feeding intake;
(2) finish after material fully reacts and pass into 0.95 ton of Trimethylamine 99 again, when feeding intake, temperature of reaction controls at 55 DEG C, stop as PH=7 feeding intake, Trimethylamine 99 feeds intake in process, reactor pressure does not allow more than 0.1Mpa, and after the logical material of Trimethylamine 99, temperature 50 C starts to stir, be incubated 3 hours, then material moves in concentration response still;
(3) make vapor pressure be stabilized in 0.3MPa, concentrate to heating material, vacuum pressure is stabilized in-0.08MPa, heating is stopped when temperature of charge reaches 115 DEG C, stir 20 minutes, then supernatant liquor moves in liquid material hold-up vessel, and the every five batches of cleanings of the sodium-chlor in reactor once;
(4) supernatant liquor adds pure water to be diluted to salts contg is less than 10 % by weight, desalination is carried out through electrodialysis appts after mixing of materials is even, the alkali solution of beet ash of output is not more than 0.5 % by weight, detect qualified after, the salts solution of output is beaten in salts solution hold-up vessel;
(5) alkali solution of beet falling film condenser concentrates, make vapor pressure be stabilized in 0.3MPa, vacuum pressure is stabilized in-0.08MPa, stops heating when temperature of charge reaches 115 DEG C, concentrated end, the alkali solution of beet after then concentrating moves in trimethyl-glycine crystallization kettle;
(6) trimethyl-glycine crystallization: the trimethyl-glycine liquid material cooling in concentrated post crystallization still, make temperature of charge be down to less than 10 DEG C, xln is separated out in a large number;
(7) trimethyl-glycine is centrifugal: carry out solid-liquid separation with whizzer, the crystallization of output trimethylglycine hydroxide, ash is not more than 0.1 % by weight, detect qualified after, the trimethylglycine hydroxide crystal produced loads in the material cycling bag of regulation, isolated liquid collecting is in liquid material holding tank, and production cycle is applied mechanically;
(8) dropped in boiling drier by trimethylglycine hydroxide crystal, temperature controls below 115 DEG C, dry 20 minutes, the crystal water in product and moisture is dried, obtains BETAINE anhydrous product.
After measured, the purity of gained BETAINE anhydrous is 99.97%, and yield is 98.6%.
Embodiment 2
(1) under normal temperature by 2 tons of water, 1.5 tons of Mono Chloro Acetic Acids, 0.84 ton of sodium carbonate drops in reactor, will note rate of feeding, be as the criterion not separate out a large amount of carbonic acid gas when feeding intake;
(2) finish after material fully reacts and pass into 0.95 ton of Trimethylamine 99 again, when feeding intake, temperature of reaction controls at 65 DEG C, stop as PH=7 feeding intake, Trimethylamine 99 feeds intake in process, reactor pressure does not allow more than 0.1Mpa, and after the logical material of Trimethylamine 99, temperature 60 C starts to stir, be incubated 3 hours, then material moves in concentration response still;
(3) make vapor pressure be stabilized in 0.3MPa, concentrate to heating material, vacuum pressure is stabilized in-0.08MPa, heating is stopped when temperature of charge reaches 115 DEG C, stir 20 minutes, then supernatant liquor moves in liquid material hold-up vessel, and the every five batches of cleanings of the sodium-chlor in reactor once;
(4) supernatant liquor adds pure water to be diluted to salts contg is less than 10 % by weight, desalination is carried out through electrodialysis appts after mixing of materials is even, the alkali solution of beet ash of output is not more than 0.5 % by weight, detect qualified after, the salts solution of output is beaten in salts solution hold-up vessel;
(5) alkali solution of beet falling film condenser concentrates, make vapor pressure be stabilized in 0.3MPa, vacuum pressure is stabilized in-0.08MPa, stops heating when temperature of charge reaches 115 DEG C, concentrated end, the alkali solution of beet after then concentrating moves in trimethyl-glycine crystallization kettle;
(6) trimethyl-glycine crystallization: the trimethyl-glycine liquid material cooling in concentrated post crystallization still, make temperature of charge be down to less than 10 DEG C, xln is separated out in a large number;
(7) trimethyl-glycine is centrifugal: carry out solid-liquid separation with whizzer, the crystallization of output trimethylglycine hydroxide, ash is not more than 0.1 % by weight, detect qualified after, the trimethylglycine hydroxide crystal produced loads in the material cycling bag of regulation, isolated liquid collecting is in liquid material holding tank, and production cycle is applied mechanically;
(8) dropped in boiling drier by trimethylglycine hydroxide crystal, temperature controls below 115 DEG C, dry 30 minutes, the crystal water in product and moisture is dried, obtains BETAINE anhydrous product.
After measured, the purity of gained BETAINE anhydrous is 99.98%, and yield is 98.3%.
Claims (1)
1. a preparation method for BETAINE anhydrous, is characterised in that and comprises the following steps:
(1) under normal temperature by 2 tons of water, 1.5 tons of Mono Chloro Acetic Acids, 0.84 ton of sodium carbonate drops in reactor, will note rate of feeding, be as the criterion not separate out a large amount of carbonic acid gas when feeding intake;
(2) finish after material fully reacts and pass into 0.95 ton of Trimethylamine 99 again, when feeding intake, temperature of reaction controls at 55-65 DEG C, stop as PH=7 feeding intake, Trimethylamine 99 feeds intake in process, reactor pressure does not allow more than 0.1Mpa, and after the logical material of Trimethylamine 99, temperature 50-60 DEG C starts to stir, be incubated 3 hours, then material moves in concentration response still;
(3) make vapor pressure be stabilized in 0.3MPa, concentrate to heating material, vacuum pressure is stabilized in-0.08MPa, heating is stopped when temperature of charge reaches 115 DEG C, stir 20 minutes, then supernatant liquor moves in liquid material hold-up vessel, and the every five batches of cleanings of the sodium-chlor in reactor once;
(4) supernatant liquor adds pure water to be diluted to salts contg is less than 10 % by weight, desalination is carried out through electrodialysis appts after mixing of materials is even, the alkali solution of beet ash of output is not more than 0.5 % by weight, detect qualified after, the salts solution of output is beaten in salts solution hold-up vessel;
(5) alkali solution of beet falling film condenser concentrates, make vapor pressure be stabilized in 0.3MPa, vacuum pressure is stabilized in-0.08MPa, stops heating when temperature of charge reaches 115 DEG C, concentrated end, the alkali solution of beet after then concentrating moves in trimethyl-glycine crystallization kettle;
(6) trimethyl-glycine crystallization: the trimethyl-glycine liquid material cooling in concentrated post crystallization still, make temperature of charge be down to less than 10 DEG C, xln is separated out in a large number;
(7) trimethyl-glycine is centrifugal: carry out solid-liquid separation with whizzer, the crystallization of output trimethylglycine hydroxide, ash is not more than 0.1 % by weight, detect qualified after, the trimethylglycine hydroxide crystal produced loads in the material cycling bag of regulation, isolated liquid collecting is in liquid material holding tank, and production cycle is applied mechanically;
(8) dropped in boiling drier by trimethylglycine hydroxide crystal, temperature controls below 115 DEG C, dry 20-30 minute, the crystal water in product and moisture is dried, obtains BETAINE anhydrous product.
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| CN105037184A (en) * | 2015-05-29 | 2015-11-11 | 韩锦超 | Preparation method of anhydrous betaine capable of preventing moisture absorption |
| CN108689868A (en) * | 2017-04-06 | 2018-10-23 | 山东瑞弘生物科技有限公司 | The preparation method of high-purity betaine |
| CN108299215A (en) * | 2018-02-22 | 2018-07-20 | 山东瑞弘生物科技有限公司 | The production method of Citrate de Betaine |
| CN112342003B (en) * | 2019-08-07 | 2022-01-07 | 沧州中润化学助剂有限公司 | Preparation method of viscoelastic surfactant for improving recovery ratio |
| CN111423334B (en) * | 2020-04-09 | 2022-12-06 | 天津大学 | A method for preparing cubic anhydrous betaine crystals |
| CN114478285A (en) * | 2022-03-16 | 2022-05-13 | 玉星生物(集团)股份有限公司 | Betaine separation and purification method |
| CN117534579A (en) * | 2023-10-12 | 2024-02-09 | 重庆中润新材料股份有限公司 | Preparation method of betaine quaternary ammonium base |
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